US2611929A - Method of producing shaped articles from artificial or synthetic fiberor film-forming materials - Google Patents

Method of producing shaped articles from artificial or synthetic fiberor film-forming materials Download PDF

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Publication number
US2611929A
US2611929A US232208A US23220851A US2611929A US 2611929 A US2611929 A US 2611929A US 232208 A US232208 A US 232208A US 23220851 A US23220851 A US 23220851A US 2611929 A US2611929 A US 2611929A
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US
United States
Prior art keywords
bath
solvent
liquid
precipitant
shaped
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US232208A
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English (en)
Inventor
Howard M Hoxie
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Solutia Inc
Original Assignee
Chemstrand Corp
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to BE512121D priority Critical patent/BE512121A/xx
Application filed by Chemstrand Corp filed Critical Chemstrand Corp
Priority to US232208A priority patent/US2611929A/en
Priority to GB12891/52A priority patent/GB716827A/en
Priority to DEC5917A priority patent/DE966316C/de
Priority to CH304354D priority patent/CH304354A/fr
Priority to FR1063170D priority patent/FR1063170A/fr
Application granted granted Critical
Publication of US2611929A publication Critical patent/US2611929A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/06—Wet spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F6/18—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S425/00—Plastic article or earthenware shaping or treating: apparatus
    • Y10S425/017—Filament stretching apparatus

Definitions

  • This invention relates to improvements in the production of synthetic or artificial fibers, films, or other shaped articles by the wet-spinning or wet-forming processes.
  • a solution of the material to be shaped is extruded into a vessel containing a suitabl setting liquid which is continuously or periodically withdrawn from the vessel, reconditioned, and returned to the extrusion vessel.
  • the present invention is concerned more particularly with wet-spinning or wet-forming proc esses in which a solution or dispersion of the fiberor film-forming material is extruded into a setting bath comprising the solvent and a precipitant in critical, controlled relative proportions which must be maintained throughout the extrusion, and has as one object to facilitate maintaining the relative proportion of solvent to precipitant in the setting bath substantially constant from the beginning to the end of the extrusion.
  • a solution or dispersion of the fiberor film-forming material is extruded into a setting bath comprising the predetermined proportion of solvent and precipitant to form the shaped article, the article is withdrawn from the bath and, prior to any drying thereof, it is washed with the preprecipitant and a minor proportion of the solvent, and liquid from this initial washing of the article is continuously delivered to the setting bath.
  • the composition of thebath may be maintained constant. Thereforefwhen operating in accordance with the invention, it is unnecessary to withdraw the setting'bath'irom the vessel in which the extrusion is performed,
  • the method of the invention can be, used for producing artificial or synthetic fibers or other shaped articles from any fiberorfilm forming material which can bedissolved 0r dispersed and wet-spun, when the shaping involves'precipitation only.
  • acetone for commerciaLsecondary, cellulose acetate and such fiber-forming vinyl resins as those resulting from the. conjoint polymerization of vinyl chloride and vinyl acetate or of vinyl "chloride and acrylonitrile and containing from' 40 to acrylonitrile in the molecule; hot-phenol 0r formamide ior polyamides; chloroform for the polyesters; and dimethylformamide, dirnethylacetamide or dimethylpropionamide for acrylonitrile polymers containing from '70 to 98% by weight of acrylonitrile in the molecule and obtaiinedby polymerizing acrylonitrile with one or moref'other monethylenically unsaturated polymerizabl subinyl chloride, vinyl monomers containing bas'i, tertiary nitrogen such as the vinylp'yridi'nes and particularly the 2-vinylpyridines, 5-vinyl"2- methylpyridine and the
  • the solvent "and dispersing agents mentioned are illustrativejfonly and other solvents or dispersing agents maybe substituted for them.
  • the precipitant selected will depend on both 5o the'fiberor film-forming material being shaped such material is dissolved or dispersed. It may be any liquid which is an extractive for the extrusion solvent or dispersing agent but inert to 4 fibers advance upwardly through the trough 6, they are washed by liquid supplied to the trough from the vessel 9 with which the trough communicates, for example, with water which may the fiber-.formingmaterial. ..When water meets 5 be heated to a temperature up to 100 C., for tnis essential requirement, water is the preferred instance: from room temperature: to 100 C.
  • a controlled portion of Vietnamese dimethylacetamide is continuously extruded into that liquid, which always comprises a mixture .asetting bath comprising a mixture of water and of the precipitant and the solvent, is continujdiniethyla'cetamide. containing the dimethylously delivered to-vessel 2 through'pipe" 14 pro- Uacetamide in a selected. proportion.
  • the rate of flow be ng conand' 70 by .volume, and the composition of the trolled and correlated with the proportion of solsetting-bath is maintained'constant by'washing vent in the bath so that the liquid introduced the fibers as they are withdrawn from the bath from vessel I3'serves to compensate for the p ewith water onwater :containing a minor propor- 'cipitant and'solvent carried from the bath by the ii tion of dimethylace'tamide, and delivering the fr hly f rmed fi r n hi W y, h r l tive 1 liquid fromthe washing step into the setting proportions of the precipitant and solvent in the bath at acontrolled rate.
  • the conditions are setting'bath' are maintained substantially con- .selected so that the composition of the setting Stantb'ath-does notvary more than 2% from the pre- V ss l 2 is provid dwith an overflow p p 6 ;.-.determined volumetric proportions and the proformaintainingthe level of the setting bath conportion of dimethylacetamide present in' the stantpand avertically adjustable overflow pipe setting bath is at least 20% by volume.
  • H associated with vessel [3 permits withdrawal .'.--.At the start of operations under any given set I of any liquid fr m th wash n st p which is'not Iofspinning conditions, the proportion of precipidelivered to vessel 21
  • the withdrawn liquid may ...tant to solvent required in the liquid from the be stored for lateruse as a setting bath.
  • washing step and the rate at which that liquid -When the spinning is conducted at room tem- ..must be delivered to the setting bath to maintain 40" perature, as is preferred, or at temperatures begtheicomposition of thebath constant, can be delow 100 C., and the washing liquid is heated, it ..termined byobservation of the-refractive index of is necessary to cool the liquid from h Washing Lathe bath; Thereafter, adjustments in the washstep-before delivering it to the bath.
  • An' advantage of the present method is that the avoridecreasing the rate of fiow of the liquid from gtheewashing step to the setting bath.
  • Suitable F apparatus .for the production of artificial or syn- N. thetic fibers or. threads in accordance with: the invention is illustrated. in the. accompanying spinning solvent is recovered from-mixtures in which it is present in'relatively-high concentration i. e., from the settirig bath or from liquid remaining after initial washing of the fibers or the like.
  • the article may be stretched prior to, during, or after the initial washing at temperatures desfibereforming.
  • material is extruded through the 0,, .spinneretl into vessel2 containing a settingbath scomprisingthe predetermined. relative proporevtionsof solvent" and precipitant; .
  • the fibers are withdrawn from the bath under the guide 3 and ,lapped-around godet 4, a thread displacing guide 5 .being ,supportedadjacentthe godet. .From
  • godet 4 the fibers are passed upwardly through the. open'trough 6 and lapped around godet 1, a
  • Z""'threaddisplacing guide 8 beingsupportedadja- --pehding on the material shaped, and may or may not be given an" after-stretch.
  • freshly-formed'fibers' of the acrylonitrile poly- -mers o1" blends' may be stretched'IOO to-300%-at temperatures up to' 100 stretched morethan 300% 0., or they may be at temperatures above cent to that godet to assist in laying the fibers.
  • the acrylonitrile polymer fibers may be I stretched between "the godets' 4 and 1 simultaneously with washing thereof with water at any temperature up to 100 C., for instance a temperature between ordinary room temperature and 100 0., v and then after-stretched at temperatures above l-' C. If the acrylonitrile polymer fibers are to be simultaneously stretched and heated to a temperature above 100 C., the godet used in-the production of shaped article's, espe- -cially fibers of the acrylonitrile polymers, which term is intended to include polyacrylonitrile, co-
  • polymers and interpolymers of a'crylonitrile with one or more other vinyl type monomers contain-. 1 ing at least 70% of acrylonitrile by weight in the polymer molecule, and blends comprising the acrylonitrile polymers.
  • the latter are those compositions obtained byblending an acrylonitrile' polymer containing, by weight in the molecule at least 70% of acrylonitrile with a copolymer of from to 70% of acrylonitrile and from'30 to 90% of a'yinyl-substituted heterocyclic tertiary amine, such as a vinylpyridine'to obtain a blend having an overall content'of the poly:
  • ' 3000 filament tow was formed by continuously extruding a spinning solution comprising a homo: geneous mixture of N,N-dimethylacetamide and 14.2% by weight of a polymer containing about 95% of acrylonitrile and about 5% of 2-vinylpyridine throughaspinneret into a setting bath at room temperature and consisting of 58% of N,N-dimethylacetamide and 42% of water, by weight, the solution being delivered through the spinneret at a rate of 1.76 lbs/minute.
  • the tow of filaments carried 0.5 lb. of N,N-dimethylacetamide per minute out of the setting bath into the trough 6. Water at about 100 C.
  • Example II Using apparatus as shown in the drawing, a 5000 filament tow was formed by continuously extruding a spinning solution comprising a. homogeneous mixture of N,N-dimethylacetamide and 14.2% of a copolymer of 95% acrylonitrile and 5% of 2-vinylpyridine, at room temperature and consisting of 58% of N,N-dimethylacetamide and 42% of water, by weight, the solution being delivered through the spinneret at a rate of 2.937 lbs. per minute.
  • the tow of filaments carried 0.834 lb. of N,N-dimethylacetamide per minute from the setting baths; into trough .6.- waterat about 100 C.
  • the yarn leaving the setting" bath comprising the solvent and precipitant contains an amount of solvent' which appreciably greater than 1.5% by weight; and ordinarily, prolonged washing would be requiredto-"reduce the solvent to less than 1.5%; However, in practicing this invention, the conditions,such as the length and width of trough 6.
  • the angle of inclination of the troughwith respect to ve'ssels 2 and 9, the rate of fiow of the washing liquid through the trough countercurrentlyto the'yarn advancing from thebath, and the -temperature of the washing liquid may be selected so that the yarn leaving the trough after the initial washing contains less than 1.5% of the-spir'ming'isolvent and additional washings are not 'neces'sary prior to stretching the yarns at temperatures above 100 C.
  • solven and solution are intended to include true solvents and solutions as well as dispersing agents and dispersions or colloidal solutions or mixtures in which the fiberor film-forming material is substantially uniformly dispersed.
  • fibers is intended to include filaments and yarns.
  • a method of forming artificial and synthetic fibers and other shaped articles which comprises continuously extruding a solution oi the material to be shaped into a setting bath comprising a mixture of the solvent and a liquid precipitant for the material to be shaped, which precipitant is anextractive for the solvent, 0on
  • a method-fas in claim -1, -Whereini:the material to.- be; shaped is a-zblend of an acrylonitrile 1 polymercontainingiby-weight in the polymer molecule, atleast 70%-:of-acrylonitrile andacoipolymer of-irom 16 to 7.0% of acryloni-trileand -..:from 30 to 9.0% of avinylpyridine.
  • the materia1 to be shaped is a blend of. an acrylonitrile polymer containing, by'weight in the polymer moleculaat least 7.0% of acrylonitrile with a copolymer of from 10 to of-acrylonitrile-and i from 30 to of a vinylpyridine.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
US232208A 1951-06-18 1951-06-18 Method of producing shaped articles from artificial or synthetic fiberor film-forming materials Expired - Lifetime US2611929A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
BE512121D BE512121A (en, 2012) 1951-06-18
US232208A US2611929A (en) 1951-06-18 1951-06-18 Method of producing shaped articles from artificial or synthetic fiberor film-forming materials
GB12891/52A GB716827A (en) 1951-06-18 1952-05-21 Improvements relating to a method for obtaining fibers or films by the wet-spinning and wet-forming processes
DEC5917A DE966316C (de) 1951-06-18 1952-05-31 Verfahren zur Aufrechterhaltung des Verhaeltnisses von Loesungsmittel zum Faellmittel im Faellbad bei der Herstellung von kuenstlichen Gebilden
CH304354D CH304354A (fr) 1951-06-18 1952-06-17 Procédé pour la fabrication d'articles extrudés, notamment de fibres et films.
FR1063170D FR1063170A (fr) 1951-06-18 1952-06-17 Procédés de préparation de fibres et films synthétiques et autres objets

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US232208A US2611929A (en) 1951-06-18 1951-06-18 Method of producing shaped articles from artificial or synthetic fiberor film-forming materials

Publications (1)

Publication Number Publication Date
US2611929A true US2611929A (en) 1952-09-30

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US232208A Expired - Lifetime US2611929A (en) 1951-06-18 1951-06-18 Method of producing shaped articles from artificial or synthetic fiberor film-forming materials

Country Status (6)

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US (1) US2611929A (en, 2012)
BE (1) BE512121A (en, 2012)
CH (1) CH304354A (en, 2012)
DE (1) DE966316C (en, 2012)
FR (1) FR1063170A (en, 2012)
GB (1) GB716827A (en, 2012)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2888317A (en) * 1953-04-10 1959-05-26 Du Pont Production of polyacrylonitrile filaments of high uniform density
US2943598A (en) * 1956-10-08 1960-07-05 Gen Electric Wire coating apparatus
US2970884A (en) * 1958-05-07 1961-02-07 Dow Chemical Co Modified acrylonitrile polymer fibers with increased shrinkability and dyeability
US2983571A (en) * 1958-04-23 1961-05-09 Dow Chemical Co Process for wet spinning and washing synthetic fibers
US3006027A (en) * 1958-06-27 1961-10-31 Spinnfaster Ag Method and apparatus for spinning and stretching viscose rayon
US3066007A (en) * 1955-07-11 1962-11-27 British Celanese Manufacture of artificial filamentary materials
US3099517A (en) * 1960-12-16 1963-07-30 Dow Chemical Co Process of treating wet-spun acrylonitrile polymer fibers
US3124631A (en) * 1961-03-22 1964-03-10 Process for providing high density dry spun
US4185063A (en) * 1975-02-04 1980-01-22 Chute Challoner R Shaping and stretching aqueous formic acid solutions of polypyrrolidone, filament and film products
WO1996006209A1 (en) * 1994-08-23 1996-02-29 Monsanto Company Acrylonitrile filament process
CN102423141A (zh) * 2011-08-03 2012-04-25 东华大学 一种采用静电纺醋酸纤维膜的香烟过滤嘴的制备方法
CN104451914A (zh) * 2014-12-09 2015-03-25 成都丽雅纤维股份有限公司 一种粘胶纤维纺丝机进酸装置
CN104451915A (zh) * 2014-12-09 2015-03-25 成都丽雅纤维股份有限公司 一种过滤式纺丝机浴槽

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2681265A (en) * 1948-11-27 1954-06-15 American Viscose Corp Spinning artificial filaments

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None *

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2888317A (en) * 1953-04-10 1959-05-26 Du Pont Production of polyacrylonitrile filaments of high uniform density
US3066007A (en) * 1955-07-11 1962-11-27 British Celanese Manufacture of artificial filamentary materials
US2943598A (en) * 1956-10-08 1960-07-05 Gen Electric Wire coating apparatus
US2983571A (en) * 1958-04-23 1961-05-09 Dow Chemical Co Process for wet spinning and washing synthetic fibers
US2970884A (en) * 1958-05-07 1961-02-07 Dow Chemical Co Modified acrylonitrile polymer fibers with increased shrinkability and dyeability
US3006027A (en) * 1958-06-27 1961-10-31 Spinnfaster Ag Method and apparatus for spinning and stretching viscose rayon
US3099517A (en) * 1960-12-16 1963-07-30 Dow Chemical Co Process of treating wet-spun acrylonitrile polymer fibers
US3124631A (en) * 1961-03-22 1964-03-10 Process for providing high density dry spun
US4185063A (en) * 1975-02-04 1980-01-22 Chute Challoner R Shaping and stretching aqueous formic acid solutions of polypyrrolidone, filament and film products
WO1996006209A1 (en) * 1994-08-23 1996-02-29 Monsanto Company Acrylonitrile filament process
CN102423141A (zh) * 2011-08-03 2012-04-25 东华大学 一种采用静电纺醋酸纤维膜的香烟过滤嘴的制备方法
CN104451914A (zh) * 2014-12-09 2015-03-25 成都丽雅纤维股份有限公司 一种粘胶纤维纺丝机进酸装置
CN104451915A (zh) * 2014-12-09 2015-03-25 成都丽雅纤维股份有限公司 一种过滤式纺丝机浴槽

Also Published As

Publication number Publication date
GB716827A (en) 1954-10-13
DE966316C (de) 1957-07-25
CH304354A (fr) 1955-01-15
FR1063170A (fr) 1954-04-30
BE512121A (en, 2012)

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